MICROCHEMICAL JOURNAL
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2025
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IF 5.1
Lingcan Kong,Haixin Chen,Qiaoyan Liu
Excessive intake bioamines is harmful to human health, and thus the development of simple, rapid and efficient detection method of bioamines in food is urgent. Herein, an unprecedented method based on a commercial molecular sieve has been developed for the determination of four bioamines (cadaverine, tyramine, histamine and tryptamine) in fruit wines by dispersive solid phase microextraction (D-μSPE) coupled to liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). The extraction process of ultra-stable Y-type molecular sieve (USY) on bioamines belongs to physisorption, and the adsorption pattern is found in good accord with the Langmuir isotherm model. Theoretical and experimental analyses are further used to explore their binding energies, binding constants, and the maximum adsorption capacity. It is found that the adsorption is driven mainly by hydrogen bonds between USY and bioamines and water molecules. Moreover, the extraction efficiency is dependent on the binding constants and the maximum adsorption capacity of USY. The optimization of adsorption-desorption process involves the USY amount, extraction time, desorption solvent, desorption time, desorption number and cyclic usage number of USY. Under the optimum conditions, the limits of detection and quantification were found in the range of 0.2–2.5 μg L −1 and 0.6–8 μg L −1 with intra-day and inter-day precision and recoveries in a fruit wine in the range of 1.3 %–7.9 % and 91 %–104 %, respectively. Owing to the efficient enrichment and edulcoration functions of USY, the method shows negligible matrix effect and is simple, rapid, and has the potential to apply in routine work.
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CLINICAL BIOCHEMISTRY
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2025
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IF 2.1
Chunyan Zhang,Nan Bai,Yanling Yang,Yuxuan Cheng,Xiyu He,Meng Wang,Honghui Zhou,Yaping Tian
Objectives Metabolic disorders in newborns can cause significant morbidity and mortality if not diagnosed and managed early. In this study, we developed and validated a reliable LC-MS/MS method to simultaneously quantify methylmalonic acid, methylcitric acid, malonic acid, ethylmalonic acid, and total homocysteine associated with metabolic disorders. Design and methods According to Clinical Laboratory Standards Institute (CLSI) guidelines, various analytical performances (i.e., precision, linearity, accuracy and reference intervals) were rigorously evaluated. Meanwhile, sample preparation, chromatographic separation and mass spectrometric detection and incorporating stable isotope-labeled internal standards were optimized. Furthermore, calibrators and quality controls were developed to ensure standardization and traceability. Results The coefficient of variations for precision were less than 10.0 %. Meanwhile, the results showed high accuracy (recoveries: 94.57 %–109.60 %) and robust linearity (R 2 > 0.9935) over clinically relevant ranges. The limits of detection and limits of quantification for all analytes were established, enabling sensitive detection of pathological elevations. Reference intervals for pediatric populations (ages 0–1 month and 2 months to 18 years) were determined, providing essential baselines for clinical interpretation. Conclusions The newly developed method demonstrated good analytical performance and offers a standardized, high-throughput solution for clinical laboratories to improve early diagnosis and personalized management of metabolic diseases.
研究领域:
临床化学
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代谢组学
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新生儿筛查
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质谱分析
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生物医学检验
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BIOMEDICAL CHROMATOGRAPHY
·
2017
·Vol. 32
·期 4
·e4156
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IF 1.613
Qing Tong,Jia Song,Guangjie Yang,Li Fan,Wei Xiong,Jianguo Fang
Reliable methods for the determination of tryptophan and its metabolites are vital to the monitoring of biochemical states during the initiation and progression of cardiovascular disease. In the present study, a single-run liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of tryptophan (Trp) and its metabolites, including kynurenine (Kyn), kynurenic acid (KA), xanthurenic acid (XA) and 5-hydroxytryptamine (5-HT), in human plasma. The plasma samples were prepared using a protein precipitation approach, and the chromatographic separation was performed by gradient elution on a C 18 column within a total analysis time of 3.5 min. The calibration ranges were 40–20,000 ng/mL for Trp, 4–2000 ng/mL for Kyn, 0.2–100 ng/mL for KA, 0.4–200 ng/mL for XA and 1–500 ng/mL for 5-HT, and the precision and accuracy were acceptable. The evaluation of recovery and internal standard-normalized matrix effect proved that the sample preparation approach was effective and the matrix effect could be negligible. The newly developed method was successfully applied to the analysis of plasma samples from healthy individuals and myocardial infarction patients. The findings suggested that the plasma concentrations of Trp, Kyn, 5-HT as well as the concentration ratios of Kyn/Trp and Trp/5-HT might serve as biomarkers for the monitoring of acute myocardial infarction.
研究领域:
临床化学
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心血管疾病
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分析化学
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CHEMISTRY & BIODIVERSITY
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2022
·Vol. 20
·期 1
·e202200574
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IF 2.745
Haixia Han,Rui Ma,Aidi Xie,Juanjuan Gao,Zhen Wang,Yi Zhao,Huanming Pang,Wei Zhang
Eleven polyphenols, classified as flavonoid glycosides, flavonoid aglycones, and phenolic acids, are important bioactive components in the capitula of Coreopsis tinctoria (CCT). Nevertheless, their full pharmacokinetic profiles have not been demonstrated simultaneously. Therefore, a liquid chromatography – tandem mass spectrometry (LC/MS/MS) method was developed in the present work and used it to study the pharmacokinetics of these 11 compounds. We performed LC/MS/MS with a gradient mobile phase composed of water containing 0.1 % formic acid and acetonitrile containing 0.1 % formic acid on a Proshell 120 SB C18 column (2.1 mm×100 mm, 2.7 μm). We achieved a good chromatographic peak shape, resolution, and mass signal response, and multiple reaction monitoring facilitated the simultaneous detection of 11 analytes. In addition, we validated the selectivity, correlation coefficient, precision, extraction recovery, matrix effects, and stability of the LC/MS/MS method to be acceptable for 11 analytes in rat plasma. Subsequently, rats were orally administered with 50 % ethanol eluent of CCT (ECCT). Nine of 11 polyphenols were absorbed quickly (except for QCD and TCA), and their plasma levels peaked within 40 min. The exposure and C max values of flavonoid glycosides and phenolic acids were lower than those of flavonoid aglycones. This is the first report to demonstrate the pharmacokinetics of 11 polyphenols in ECCT, which may play an important role in future studies of the bioactive components of ECCT and their bioactive mechanisms. Graphical
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PHYTOMEDICINE
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2022
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IF 6.656
Wanqian Peng,Zhiqiang Li,Dingji Cai,Xiaocui Yi,Ji Yue (Jeff) Zhang,Guoyue Zhong,Hui Ouyang,Yulin Feng,Shilin Yang
Background Pinnatifolone A is a typical sesquiterpenoid and the primary active ingredient of Syringa oblata Lindl., has potent anti-inflammatory activity. However, Pinnatifolone A pharmacokinetic and metabolites analysis investigations in male and female rats, as well as its in vitro stability in male and female rat liver microsomes , have not been evaluated and compared. Purpose To investigate preclinical pharmacokinetic and metabolite in both genders, confirm gender differences, and provide usable information for the development of clinical applications. Methods A quick, precise, and sensitive LC-MS/MS method was created and effectively used to determine the pharmacokinetics of oral (140 mg/kg) and intravenous (6.3 mg/kg) Pinnatifolone A in male and female rats, in vitro Pinnatifolone A elimination studies in male and female rat liver microsomes. Following that, a UHPLC-Q-TOF-MS/MS technique was established to identify the metabolic profiles of Pinnatifolone A obtained from rat plasma and excreta. Results In the current study, we established for the first time an LC-MS/MS method for the quantitation of Pinnatifolone A with acceptable linearity and selectivity, recovery and matrix effect, accuracy and precision. The absolute oral bioavailability of Pinnatifolone A was approximately 30.36% in female rats, the clearance (CL) was 20.99±3.33 l/h/kg in female rats and 472.37±437.31 l/h/kg in male rats. This difference in rat genders may pertain to the sex-specific expression of hepatic enzymes as demonstrated in the metabolic stability evaluation in the present research; the male rats exhibited higher CL int(mic) (158.83±9.57 μl/min/mg protein) than female rats (76.47±7.90 μl/min/mg protein) liver microsomes, indicating higher Pinnatifolone A clearance in male rats. Twenty-four metabolites were detected and identified in female and male rats; N-acetylcysteine conjugation metabolite was the most abundant metabolites in both rat feces and urine. Furthermore, male and female rats had significantly different levels of the N-acetylcysteine conjugation metabolite. Hydrogenation metabolite was particular to female rats both in rat fecal and urine. Glucuronide conjugation metabolite was the predominant metabolite in rat plasma, and its amount in female rats was double that of male rats. Conclusions The present research is the first to report the preclinical pharmacokinetics and metabolites of Pinnatifolone A in male and female rats, confirming the gender-based differences. The findings provide a comprehensive overview for further understanding of the pharmacokinetic and metabolic characteristics of Pinnatifolone A and serve as a guide for its future development and utilization.
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Frontiers in Veterinary Science
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2023
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IF 3.2
Shiting Xie,Yixing Lu,Jun Wang,Changcheng Lin,Peiyu Ye,Xiaolin Liu,Wenguang Xiong,Zhenling Zeng,Dongping Zeng
Introduction Milbemycin oxime (MBO) and praziquantel (PZQ) have a broad spectrum of biological activity and are commonly used to treat the parasitic infection in the veterinary clinic. In this study, a fast and efficient LC-MS/MS method was established and validated for the simultaneous determination of MBO, PZQ, cis-4-hydroxylated-PZQ (C-4-OH-PZQ) and trans-4-hydroxylated-PZQ (T-4-OH-PZQ) and in cat plasma. Methods Extraction of analytes and internal standards from cat plasma by acetonitrile protein precipitation, allows rapid processing of large batches of samples. MBO, PZQ, C-4-OH-PZQ, T-4-OH-PZQ, and internal standard (IS) were eluted for 13.5 min on a C 18 column with a 0.1% formic acid water/acetonitrile mixture as the mobile phase. Results Results showed that the method had good precision, accuracy, recovery, and linearity. The linearity range was 2.5–250 ng/mL for MBO, and 10–1000 ng/mL for PZQ, C-4-OH-PZQ, and T-4-OH-PZQ. The intra-day and inter-day precision CV values of the tested components were within 15%. The extraction recoveries of the four components ranged from 98.09% to 107.46%. The analytes in plasma remained stable for 6 h at room temperature, 26 h in the autosampler (4 °C), after freeze–thaw (−20°C) cycles, and 60 days in a −20°C freezer. Method sensitivity sufficed for assessing pharmacokinetic parameters of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ in plasma samples with LLOQ of 2.5 ng/mL for MBO and 10 ng/mL for PZQ, C-4-OH-PZQ, and T-4-OH-PZQ. Conclusion In this study, a selective and sensitive LC-MS/MS method for the simultaneous quantification of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ in cat plasma was developed and validated.This method had been successfully applied to evaluate the pharmacokinetics of MBO, PZQ, C-4-OH-PZQ, and T-4-OH-PZQ after a single oral administration of 8 mg MBO and 20 mg PZQ in cats.
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Frontiers in Chemistry
·
2019
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IF 3.782
Chen Lizhu,Yu Yingjia,Duan Gengli,Wang Xin,Shen Baohua,Xiang Ping
Objective: Chiral analysis is a crucial method to differentiate selegiline intake from drug abuse. A dried urine spot (DUS) analytical method based on spotting urine samples (10 μL) onto dried spot collection cards, and followed by air-drying and extraction, was developed and validated for the determination of selegiline, desmethylselegiline, R/S-methamphetamine, and R/S-amphetamine.Methods: Methanol (0.5 mL) was found to be the ideal extraction solvent for target extraction from DUSs under orbital-horizontal stirring on a lateral shaker at 1,450 rpm for 30 min. Determinations were performed by direct electrospray ionization tandem mass spectrometry (ESI-MS/MS) under positive electrospray ionization conditions using multiple reaction monitoring mode. The chromatographic system consisted of a ChirobioticTM V2 column (2.1 × 250 mm, 5 μm) and a mobile phase of methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide.Results and conclusions: The calibration curves were linear from 50 to 5,000 ng/mL, with r > 0.995 for all analytes, imprecisions ≤ 15% and accuracies between −11.4 and 11.7%. Extraction recoveries ranged from 48.6 to 105.4% with coefficients of variation (CV) ≤ 13.7%, and matrix effects ranged from 45.4 to 104.1% with CV ≤ 10.3%. The lower limit of quantification was 50 ng/mL for each analyte. The present method is simple, rapid (accomplished in 12 min), sensitive, and validated by a pharmacokinetic study in human urine collected after a single oral administration of SG.
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Forensic Toxicology
·
2024
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IF 2.8
Zhang Xiaolong,Chen Yuxuan,Liu Jinlei,Wang Mengchao,Dai Yinyin,Zhao Kundi,Gu Jie,Zhang Huimin,Wurita Amin,Hasegawa Koutaro
Purpose Distribution and abuse of imidazole-derived γ-aminobutyric acid (GABA) agonists, such as etomidate and metomidate, and their analogs have been encountered frequently especially in China. The aim of this study was to identify etomidate, metomidate, propoxate, and isopropoxate more accurately by establishing a gas chromatography–mass spectrometry (GC–MS) and liquid chromatography tandem mass spectrometry (LC–MS/MS) method and applying it to real forensic cases. Methods One mg of the seized powder was dissolved in 1 mL of methanol, and subjected to GC–MS and LC–MS/MS. Hair samples were washed and cut into approximately 2 mm sections, then ground to powder by a low-temperature grinder. Twenty mg of the hair powder was extracted with 1 mL of methanol, and the supernatant was subjected to LC–MS/MS. Results Etomidate, metomidate, propoxate, and isopropoxate were chromatographically separated and each mass spectrum was obtained by GC–MS. For LC–MS/MS, tested validation data were all satisfactory. The seized powder samples contained isopropoxate, with an approximate content of 30.9%. Etomidate, etomidate acid, metomidate, and isopropoxate could be determined in the submitted hairs, ranging from 2.89 to 8.09 ng/mg, 0.0591–0.177 ng/mg, 0.342–2.77 ng/mg, and 33.2–130 ng/mg, respectively. Conclusions Mass spectra and ion chromatograms of etomidate, metomidate, isopropoxate, and propoxate were obtained by GC–MS. We have also established a simultaneous and reliable analytical method for etomidate, etomidate acid, metomidate, and isopropoxate in human hair by LC–MS/MS. This is the first report to present analytical results of a novel imidazole-derived GABA agonist isopropoxate in drug abuse cases.
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TALANTA
·
2024
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IF 5.6
Xianjing Li,Minlu Cheng,Yiya Wang,Chang Shu,Bingjie Zou,Qinxin Song,Li Ding
Recently, peptide-drug conjugate (PDC) has become the most promising conjugated drug for tumor therapy after antibody-drug conjugate due to stronger tumor penetration capacity and lower immunogenicity . CBP-1018 was a PDC with dual-ligand conjugated to MMAE via a cleavable linker (MC-Val-Cit-PABC) that can be lysed by cathepsins B. In this study, two specific LC-MS/MS methods were developed and validated for the determination of CBP-1018 and its metabolite MMAE in human plasma. To prevent the cleavable MC-Val-Cit-PABC linker from degradation, a protease inhibitor (cOmplete solution) was added to the pre-cooled vacuum tubes and the separated plasma samples. The assays involved the pretreatment of CBP-1018 by protein precipitation with H 2 O-ACN (1:9, v / v ) and the extraction of MMAE by liquid-liquid extraction with ethyl acetate under alkaline condition to eliminate the interference of CBP-1018 on MMAE. The two analytes showed good linearities over the calibration ranges (R 2 ≥ 9980). Both accuracy and precision met the acceptance criteria. The validated methods were successfully applied to the phase I dose-escalation study of CBP-1018 injection in Chinese patients with solid tumors to evaluate the pharmacokinetic properties of CBP-1018 and MMAE. The results showed that CBP-1018 was eliminated immediately after injection and MMAE reached the maximum exposure at approximately 2 h after infusion. The maximum concentration of MMAE did not exceed 20.0 ng/mL, suggesting that the off-target toxicity of CBP-1018 injection was controllable.
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Analytical Methods
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2017
·Vol. 9
·期 36
·5281-5292
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IF 1.9
Sheng-Dong Pan,Mei-Jun Ye,Guo-Sheng Gao,Qian He,Li Wang,Xiao-Hong Chen,Qiao-Li Qiu,Mi-Cong Jin
In this paper, a monodisperse, well-defined core–shell magnetic molecularly-imprinted polymer (MD-CS-MMIP) was controllably synthesized via modified precipitation polymerization and used as a magnetic solid-phase extraction adsorbent for the simultaneous determination of six trace mycotoxins in rice samples. The as-prepared MD-CS-MMIP was fully characterized by SEM, TEM, XRD, and TG-DTG. This study is particularly concerned with the influence of the amount of oleic acid used for MD-CS-MMIP synthesis on the material morphology, components, and adsorption efficiency. The results reveal that the modification of oleic acid on the Fe3O4 surface could improve the monodispersion of core–shell MD-CS-MMIP. Moreover, MD-CS-MMIP was used as a magnetic solid-phase extraction adsorbent for the determination of six mycotoxin residues in rice samples, and the adsorption and desorption conditions of MD-CS-MMIP toward mycotoxins were optimized to obtain the highest adsorption capacity, selectivity, and desorption efficiency. Under optimal conditions, the limits of quantitation (LOQs) of the developed method toward the six mycotoxins range from 0.003 μg kg−1 to 0.01 μg kg−1. The developed method was successfully used for the determination of mycotoxins in rice samples, with recoveries in the range of 86.3 to 103.1%.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
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IF 2.8
Ninghong Li,Lu Liu,Dong Liu,Hengyi Yu,Guangjie Yang,Lihui Qiu,Yufei Chen,Dong Xiang,Xuepeng Gong
Tyrosine kinase inhibitors (TKIs) and triazole antifungals are the first-line drugs for treating chronic myeloid leukemia (CML) and fungal infections, respectively, but both suffer from large exposure differences and narrow therapeutic windows. Moreover, these two types of drugs are commonly used together in CML patients with fungal infections. Multiple studies and guidelines have suggested the importance of therapeutic drug monitoring (TDM) of TKIs and triazoles. Currently, methods for the simultaneous determination of both types of drugs are limited. We developed a simple, rapid, and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous quantification of three commonly used TKIs (imatinib, dasatinib, and nilotinib) and three commonly used triazoles (voriconazole, itraconazole, and posaconazole) in human plasma. The analytes were eluted on a Welch XB-C 18 analytical column (50 × 2.1 mm, 5 µm) at 0.7 mL/min, using a gradient elution of 10 mM ammonium formate (A) and methanol–acetonitrile-isopropanol (80:10:10, v / v / v ) containing 0.2 % formic acid (B) with a total analysis time of 3.5 min. The calibration curves were linear over the range from 20 to 4000 ng/mL for imatinib and nilotinib, from 2 to 400 ng/mL for dasatinib, and from 50 to 10,000 ng/mL for voriconazole, itraconazole, and posaconazole. Selectivity, accuracy, precision, recovery, matrix effect, and stability all met the validation requirements. The method was successfully used for TDM in CML patients who co-treated with both TKIs and triazoles. Drug-drug interaction analysis between TKIs and triazoles showed that a significant positive correlation was observed between imatinib and voriconazole, as well as dasatinib and voriconazole. Therefore, this method can be well applied in clinical TDM for patients receiving TKIs, triazoles, or both simultaneously.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2014
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IF 2.829
Feng Chen,Hai-Long Li,Yin-Feng Tan,Yong-Hui Li,Wei-Yong Lai,Wei-Wei Guan,Jun-Qing Zhang,Yuan-Sheng Zhao,Zhen-Miao Qin
Alpinia oxyphylla (Yizhi) capsularfruits are commonly used in traditional medicine. Pharmacological studies have demonstrated that A. oxyphylla capsularfruits have some beneficial roles. Besides volatile oil, sesquiterpenes, diarylheptanoids and flavonoids are main bioactive constituents occurring in the Yizhi capsularfruits. The representative constituents include tectochrysin, izalpinin, chrysin, apigenin-4′,7-dimethylether, kaempferide, yakuchinone A, yakuchinone B, oxyphyllacinol and nootkatone. Their content levels in the fruit and its pharmaceutical preparations have been reported by our group. The nine phytochemicals are also the major components present in the Yizhi alcoholic extracts, which have anti-diarrheal activities. However, the fates of these constituents in the body after oral or intravenous administration remain largely unknown. In the present study, we focus on these phytochemicals albeit other concomitant compounds. The chemicals and their metabolites in rat plasma were identified using liquid chromatography/tandem mass spectrometry with selected reaction monitoring mode after orally administered Yizhi extract to rats. Rat plasma samples were treated by methanol precipitation, acidic or enzymatic hydrolysis. This target analysis study revealed that: (1) low or trace plasma levels of parent chemicals were measured after p.o. administration of Yizhi extract, Suoquan capsules and pills to rats; (2) flavonoids and diarylheptanoids formed mainly monoglucuronide metabolites; however, diglucuronide metabolites for chrysin, izalpinin and kaempferide were also detected; (3) metabolic reduction of Yizhi diarylheptanoids occurred in rats. Yakuchinone B was reduced to yakuchinone A and then to oxyphyllacinol in a stepwise manner and subsequently glucuronidated by UDP-glucuronosyl transferase. Further research is needed to characterize the UDP-glucuronosyl transferase and reductase involved in the biotransformation of Yizhi chemicals.
研究领域:
药理学
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分析化学
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危险品化学品经营许可证（带存储）